阅读说明：本技术 一种抗菌美白洁牙剂及其制备方法 (Antibacterial whitening dentifrice and preparation method thereof ) 是由 岑汉林 于 2021-02-26 设计创作，主要内容包括：本发明公开了一种抗菌美白洁牙剂及其制备方法,所述洁牙剂按重量份数计包括以下成分：纤维素气凝胶24～35份、丙二醇10～16份、甘油15～22份、去离子水15～25份、过氧化镁2～4份、过氧化钙1.5～3份和甜味剂8～14份、增稠剂2～5份、调味剂4～6份、氟化钾1～2.5份、羧甲基纤维素6～11份和柠檬酸锌8～14份。其制备方法包括将甘油、丙二醇和去离子水混合均匀然后加入纤维素气凝胶和增稠剂,在室温条件下以600～800r/min的转速搅拌20～30min,真空干燥,和过氧化镁、过氧化钙、甜味剂、调味剂、氟化钾、羧甲基纤维素和柠檬酸锌混合研磨搅拌混合,得到所述洁牙剂。(The invention discloses an antibacterial whitening dentifrice and a preparation method thereof, wherein the dentifrice comprises the following components in parts by weight: 24-35 parts of cellulose aerogel, 10-16 parts of propylene glycol, 15-22 parts of glycerol, 15-25 parts of deionized water, 2-4 parts of magnesium peroxide, 1.5-3 parts of calcium peroxide, 8-14 parts of a sweetening agent, 2-5 parts of a thickening agent, 4-6 parts of a flavoring agent, 1-2.5 parts of potassium fluoride, 6-11 parts of carboxymethyl cellulose and 8-14 parts of zinc citrate. The preparation method comprises the steps of uniformly mixing glycerol, propylene glycol and deionized water, then adding cellulose aerogel and a thickening agent, stirring at the rotating speed of 600-800 r/min for 20-30 min at room temperature, drying in vacuum, mixing with magnesium peroxide, calcium peroxide, a sweetening agent, a flavoring agent, potassium fluoride, carboxymethyl cellulose and zinc citrate, grinding, stirring and mixing to obtain the dentifrice.)

1. An antibacterial whitening dentifrice is characterized by comprising the following components in parts by weight: 24-35 parts of cellulose aerogel, 10-16 parts of propylene glycol, 15-22 parts of glycerol, 15-25 parts of deionized water, 2-4 parts of magnesium peroxide, 1.5-3 parts of calcium peroxide, 8-14 parts of a sweetening agent, 2-5 parts of a thickening agent, 4-6 parts of a flavoring agent, 1-2.5 parts of potassium fluoride, 6-11 parts of carboxymethyl cellulose and 8-14 parts of zinc citrate;

the thickening agent is self-made modified corn starch and is prepared by the following method:

(1) grinding corn starch through a mesh screen of 800-1000 meshes, adding the corn starch into distilled water, stirring uniformly to be viscous, adding carboxymethyl chitosan and amorphous calcium phosphate, and stirring and mixing uniformly at room temperature, wherein the mass ratio of the corn starch to the carboxymethyl chitosan to the amorphous calcium phosphate is (10-15): 2-4): 1.6-3.5;

(2) and (2) adding medium-temperature amylase into the viscous liquid obtained in the step (1), heating to 65-75 ℃, stirring for 2-4 hours, standing for 1-2 hours at the temperature, heating to 95-98 ℃, and stirring for 10-20 minutes to obtain the self-made modified starch.

2. The antibacterial whitening dentifrice of claim 1, wherein the cellulose aerogel is prepared by the method comprising:

the method comprises the following steps: adding sodium hydroxide and urea into deionized water, stirring for dissolving, then freezing to the temperature of-13 to-15 ℃ for 20-35 min, standing, heating to room temperature, then carrying out magnetic stirring, slowly adding microcrystalline cellulose during stirring, rapidly stirring for dissolving, and continuing stirring for 2-3 h when the temperature is reduced to 0 ℃ to obtain a microcrystalline cellulose solution;

step two: adding hydroxyapatite nanoparticles into deionized water, ultrasonically stirring for 1-3 hours to obtain hydroxyapatite dispersion, then adding the hydroxyapatite dispersion into a stirred microcrystalline cellulose solution, continuously stirring, adding a cross-linking agent, stirring for 45-60 min under the ice-water bath condition, then carrying out cross-linking reaction for 2-3 hours at 55-60 ℃, cooling, and freeze-drying with liquid nitrogen for 5-8 hours to obtain the cellulose aerogel.

3. The method of preparing an antibacterial whitening dentifrice according to claim 1, wherein the method of preparing the dentifrice comprises the steps of:

s1: uniformly mixing glycerol, propylene glycol and deionized water, then adding cellulose aerogel and a thickening agent, stirring at the room temperature at the rotating speed of 600-800 r/min for 20-30 min, and carrying out vacuum drying;

s2: and (4) mixing, grinding and mixing the dried substance obtained in the step (S1) with magnesium peroxide, calcium peroxide, a sweetening agent, a flavoring agent, potassium fluoride, carboxymethyl cellulose and zinc citrate to obtain the dentifrice.

4. The antibacterial whitening dentifrice of claim 2, wherein the cross-linking agent is epichlorohydrin.

5. The antibacterial whitening dentifrice of claim 2, wherein the ratio by mass of the sodium hydroxide, urea and microcrystalline cellulose is (1-1.6): (1.35-2.45): (0.96-1.54).

6. The antibacterial whitening dentifrice according to claim 2, wherein the volume ratio of the microcrystalline cellulose solution to the hydroxyapatite dispersion is (2.6-3.2) to (0.85-1.12).

7. The antibacterial whitening dentifrice according to claim 2, wherein the mass ratio of the cross-linking agent to the microcrystalline cellulose is (0.2-0.28): (1-2.2).

Technical Field

The invention belongs to the technical field of tooth cleaning agents, and particularly relates to an antibacterial whitening tooth cleaning agent and a preparation method thereof.

Background

In China, teeth discoloring caused by various reasons such as dental fluorosis, tetracycline pigmentation, smoking and the like is very common. With the increasing living standard of people, the tooth whitening technology is more and more emphasized in recent years. The traditional method for cleaning teeth adopts a hydrogen peroxide rinsing method, which not only needs to visit hospitals for many times and is expensive, but also causes damage to enamel to different degrees.

Dentifrices are used to clean teeth, and in addition to plaque from tooth surfaces, toothpastes help to remove food particles and tooth discoloration caused by substances such as tobacco, tea or wine, and toothpastes also polish teeth. Acidic beverages and desserts can cause dental erosion, for example, by attacking the enamel that coats and protects the teeth. Furthermore, tobacco-based products and beverages such as coffee and tea stain teeth and thus cause a smile that is often unattractive.

The oral cavity contains more bacteria which affect oral health, such as group A streptococcus and anaerobic streptococcus, and in addition, Staphylococcus epidermidis, Neisseria, Lactobacillus, spirochete, Candida, etc. Traditional dentifrices generally have only whitening and cleaning effects and cannot effectively inhibit the generation of oral bacteria.

Disclosure of Invention

Aiming at the problems that the prior dentifrice has only whitening and cleaning effects and lacks the effect of inhibiting oral bacteria, the invention aims to provide an antibacterial whitening dentifrice which comprises the following components in parts by weight: 24-35 parts of cellulose aerogel, 10-16 parts of propylene glycol, 15-22 parts of glycerol, 15-25 parts of deionized water, 2-4 parts of magnesium peroxide, 1.5-3 parts of calcium peroxide, 8-14 parts of a sweetening agent, 2-5 parts of a thickening agent, 4-6 parts of a flavoring agent, 1-2.5 parts of potassium fluoride, 6-11 parts of carboxymethyl cellulose and 8-14 parts of zinc citrate.

Preferably, the thickener is self-made modified corn starch and is prepared by the following method:

(1) grinding corn starch through a mesh screen of 800-1000 meshes, adding the ground corn starch into distilled water, stirring uniformly to be viscous, adding carboxymethyl chitosan and amorphous calcium phosphate, and stirring and mixing uniformly at room temperature, wherein the mass ratio of the corn starch to the carboxymethyl chitosan to the amorphous calcium phosphate is (10-15): 2-4): 1.6-3.5.

(2) And (2) adding medium-temperature amylase into the viscous liquid obtained in the step (1), heating to 65-75 ℃, stirring for 2-4 hours, standing for 1-2 hours at the temperature, heating to 95-98 ℃, and stirring for 10-20 minutes to obtain the self-made modified starch.

The invention also aims to provide a preparation method of the antibacterial whitening dentifrice, which comprises the following steps:

s1: uniformly mixing glycerol, propylene glycol and deionized water, then adding cellulose aerogel and a thickening agent, stirring at the rotating speed of 600-800 r/min for 20-30 min at room temperature, and drying in vacuum.

S2: and (4) mixing, grinding and mixing the dried substance obtained in the step (S1) with magnesium peroxide, calcium peroxide, a sweetening agent, a flavoring agent, potassium fluoride, carboxymethyl cellulose and zinc citrate to obtain the dentifrice.

Preferably, the cellulose aerogel is prepared by the following method:

the method comprises the following steps: adding sodium hydroxide and urea into deionized water, stirring for dissolving, then freezing to the temperature of-13 to-15 ℃ for 20-35 min, standing, heating to room temperature, then carrying out magnetic stirring, slowly adding microcrystalline cellulose during stirring, rapidly stirring for dissolving, and continuing stirring for 2-3 h when the temperature is reduced to 0 ℃ to obtain a microcrystalline cellulose solution.

Step two: adding hydroxyapatite nanoparticles into deionized water, ultrasonically stirring for 1-3 hours to obtain hydroxyapatite dispersion, then adding the hydroxyapatite dispersion into a stirred microcrystalline cellulose solution, continuously stirring, adding a cross-linking agent, stirring for 45-60 min under the ice-water bath condition, then carrying out cross-linking reaction for 2-3 hours at 55-60 ℃, cooling, and freeze-drying with liquid nitrogen for 5-8 hours to obtain the cellulose aerogel.

More preferably, the crosslinking agent is epichlorohydrin.

More preferably, the mass ratio of the sodium hydroxide, the urea and the microcrystalline cellulose is (1-1.6): (1.35-2.45): 0.96-1.54).

More preferably, the volume ratio of the microcrystalline cellulose solution to the hydroxyapatite dispersion is (2.6-3.2): (0.85-1.12).

More preferably, the mass ratio of the cross-linking agent to the microcrystalline cellulose is (0.2-0.28): (1-2.2).

The flavoring agent used in the present invention is a sweetening agent known in the art, such as xylitol, aspartame, stevia and the like.

Compared with the prior art, the invention has the following beneficial effects:

1. according to the invention, the cellulose aerogel prepared from microcrystalline cellulose and hydroxyapatite is used as a dentifrice additive, the cellulose aerogel has good biocompatibility and excellent adsorption performance, and can adsorb dirt on the surface of teeth in the process of cleaning the teeth, wherein the hydroxyapatite has a whitening function on the teeth, but the hydroxyapatite is directly used in the prior art, and cannot well play a whitening effect due to large particle size, so that the particle size of the hydroxyapatite is reduced to a certain extent, and the whitening effect of the dentifrice is effectively improved.

2. According to the invention, the modified self-made starch is used as a thickening agent, so that the viscosity of the dentifrice can be improved, a protective film can be formed on the surface of teeth after the dentifrice is pressed at home, the protective film can protect the teeth, and the self-made modified starch and the cellulose aerogel have good cationic accommodation property after being compounded, and generate surface adsorption and ion exchange on cations, so that an excellent antibacterial effect is achieved.

Detailed Description

The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Example 1

A preparation method of an antibacterial whitening dentifrice specifically comprises the following steps:

the dentifrice comprises the following components in parts by weight: 24 parts of cellulose aerogel, 10 parts of propylene glycol, 15 parts of glycerol, 15 parts of deionized water, 2 parts of magnesium peroxide, 1.5 parts of calcium peroxide, 8 parts of sweetener, 2 parts of thickener, 4 parts of xylitol, 1 part of potassium fluoride, 6 parts of carboxymethyl cellulose and 8-14 parts of zinc citrate.

The thickener is self-made modified corn starch and is prepared by the following method:

(1) grinding corn starch, sieving with a 800-mesh sieve, adding into distilled water, stirring to obtain a viscous state, adding carboxymethyl chitosan and amorphous calcium phosphate, and stirring and mixing at room temperature, wherein the mass ratio of the corn starch to the carboxymethyl chitosan to the amorphous calcium phosphate is 10:2: 1.6.

(2) And (2) adding medium-temperature amylase into the viscous liquid obtained in the step (1), heating to 65 ℃, stirring for 2 hours, standing at the temperature for 1 hour, heating to 95 ℃, and stirring for 10 minutes to obtain the self-made modified starch.

The cellulose aerogel is prepared by the following method:

the method comprises the following steps: adding sodium hydroxide and urea into deionized water, stirring for dissolving, then freezing to-13 ℃ for 20min, standing, heating to room temperature, then carrying out magnetic stirring, slowly adding microcrystalline cellulose during stirring, rapidly stirring for dissolving, and continuing stirring for 2h when the temperature is increased to 0 ℃ to obtain a microcrystalline cellulose solution, wherein the mass ratio of the sodium hydroxide to the urea to the microcrystalline cellulose is 1:1.35: 0.96.

Step two: adding hydroxyapatite nanoparticles into deionized water, carrying out ultrasonic stirring for 1-3 h to obtain hydroxyapatite dispersion, then adding the hydroxyapatite dispersion into a stirred microcrystalline cellulose solution, continuing stirring, wherein the volume ratio of the microcrystalline cellulose solution to the hydroxyapatite dispersion is 2.6:0.85, adding a cross-linking agent epichlorohydrin, stirring for 45min under the condition of ice-water bath, carrying out cross-linking reaction for 2h at 55 ℃, cooling, and carrying out liquid nitrogen freeze drying for 5h to obtain cellulose aerogel, wherein the mass ratio of the cross-linking agent epichlorohydrin to the microcrystalline cellulose is 0.2: 1.

The preparation method of the dentifrice comprises the following steps:

s1: mixing glycerol, propylene glycol and deionized water uniformly, adding cellulose aerogel and thickener, stirring at room temperature at a rotation speed of 600r/min for 20min, and vacuum drying.

S2: and (4) mixing, grinding and stirring the dried substance obtained in the step (S1), magnesium peroxide, calcium peroxide, a sweetening agent, xylitol, potassium fluoride, carboxymethyl cellulose and zinc citrate to obtain the dentifrice.

Example 2

A preparation method of an antibacterial whitening dentifrice specifically comprises the following steps:

the dentifrice comprises the following components in parts by weight: 35 parts of cellulose aerogel, 16 parts of propylene glycol, 22 parts of glycerol, 25 parts of deionized water, 4 parts of magnesium peroxide, 3 parts of calcium peroxide, 14 parts of sweetening agent, 5 parts of thickening agent, 6 parts of aspartame, 2.5 parts of potassium fluoride, 11 parts of carboxymethyl cellulose and 14 parts of zinc citrate.

The thickener is self-made modified corn starch and is prepared by the following method:

(1) grinding corn starch, sieving with a 1000-mesh sieve, adding into distilled water, stirring to obtain a viscous state, adding carboxymethyl chitosan and amorphous calcium phosphate, and stirring and mixing at room temperature, wherein the mass ratio of the corn starch to the carboxymethyl chitosan to the amorphous calcium phosphate is 15:4: 3.5.

(2) And (2) adding medium-temperature amylase into the viscous liquid obtained in the step (1), heating to 75 ℃, stirring for 4 hours, standing at the temperature for 2 hours, heating to 98 ℃, and stirring for 20 minutes to obtain the self-made modified starch.

The cellulose aerogel is prepared by the following method:

the method comprises the following steps: adding sodium hydroxide and urea into deionized water, stirring for dissolving, then freezing to-15 ℃ for 35min, standing, heating to room temperature, then carrying out magnetic stirring, slowly adding microcrystalline cellulose during stirring, rapidly stirring for dissolving, and then continuously stirring for 3h when the temperature is increased to 0 ℃ to obtain a microcrystalline cellulose solution, wherein the mass ratio of the sodium hydroxide to the urea to the microcrystalline cellulose is 1.6:2.45: 1.54.

Step two: adding hydroxyapatite nanoparticles into deionized water, carrying out ultrasonic stirring for 3 hours to obtain hydroxyapatite dispersion, then adding the hydroxyapatite dispersion into a stirred microcrystalline cellulose solution, continuously stirring, wherein the volume ratio of the microcrystalline cellulose solution to the hydroxyapatite dispersion is 3.2:1.12, adding a cross-linking agent epichlorohydrin, stirring for 60 minutes under the condition of ice-water bath, carrying out cross-linking reaction for 2-3 hours at 60 ℃, cooling, and carrying out liquid nitrogen freeze drying for 8 hours to obtain cellulose aerogel, wherein the mass ratio of the cross-linking agent epichlorohydrin to the microcrystalline cellulose is 0.28: 2.2.

The preparation method of the dentifrice comprises the following steps:

s1: mixing glycerol, propylene glycol and deionized water uniformly, adding cellulose aerogel and thickener, stirring at room temperature at 800r/min for 30min, and vacuum drying.

S2: and (4) mixing, grinding and stirring the dried substance obtained in the step (S1), magnesium peroxide, calcium peroxide, a sweetening agent, aspartame, potassium fluoride, carboxymethyl cellulose and zinc citrate to obtain the dentifrice.

Example 3

A preparation method of an antibacterial whitening dentifrice specifically comprises the following steps:

the dentifrice comprises the following components in parts by weight: 30 parts of cellulose aerogel, 14 parts of propylene glycol, 19 parts of glycerol, 20 parts of deionized water, 3 parts of magnesium peroxide, 2 parts of calcium peroxide, 10 parts of sweetener, 4 parts of thickener, 5 parts of stevia rebaudiana, 2 parts of potassium fluoride, 9 parts of carboxymethyl cellulose and 11 parts of zinc citrate.

The thickener is self-made modified corn starch and is prepared by the following method:

(1) grinding corn starch, sieving with a 900-mesh sieve, adding into distilled water, stirring to obtain a viscous state, adding carboxymethyl chitosan and amorphous calcium phosphate, and stirring and mixing at room temperature, wherein the mass ratio of the corn starch to the carboxymethyl chitosan to the amorphous calcium phosphate is 13:3: 2.7.

(2) And (2) adding medium-temperature amylase into the viscous liquid obtained in the step (1), heating to 70 ℃, stirring for 3 hours, standing at the temperature for 1.5 hours, heating to 96 ℃, and stirring for 15 minutes to obtain the self-made modified starch.

The cellulose aerogel is prepared by the following method:

the method comprises the following steps: adding sodium hydroxide and urea into deionized water, stirring for dissolving, then freezing to-14 ℃ for 30min, standing, heating to room temperature, then carrying out magnetic stirring, slowly adding microcrystalline cellulose during stirring, rapidly stirring for dissolving, and continuing stirring for 2.5h when the temperature is increased to 0 ℃ to obtain a microcrystalline cellulose solution, wherein the mass ratio of the sodium hydroxide to the urea to the microcrystalline cellulose is 1.4:2.03: 1.32.

Step two: adding hydroxyapatite nanoparticles into deionized water, carrying out ultrasonic stirring for 2 hours to obtain hydroxyapatite dispersion, then adding the hydroxyapatite dispersion into a stirred microcrystalline cellulose solution, continuously stirring, wherein the volume ratio of the microcrystalline cellulose solution to the hydroxyapatite dispersion is 2.9:1.04, adding a cross-linking agent epichlorohydrin, stirring for 50min under the condition of ice-water bath, carrying out cross-linking reaction for 2.5 hours at 60 ℃, cooling, and carrying out liquid nitrogen freeze drying for 7 hours to obtain cellulose aerogel, wherein the mass ratio of the cross-linking agent epichlorohydrin to the microcrystalline cellulose is 0.25: 1.6.

The preparation method of the dentifrice comprises the following steps:

s1: mixing glycerol, propylene glycol and deionized water uniformly, adding cellulose aerogel and thickener, stirring at room temperature at a rotation speed of 700r/min for 25min, and vacuum drying.

S2: and (4) mixing, grinding and stirring the dried substance obtained in the step (S1), magnesium peroxide, calcium peroxide, a sweetening agent, stevia rebaudiana, potassium fluoride, carboxymethyl cellulose and zinc citrate to obtain the dentifrice.

Examples of the experiments

Performance test 1-bacteriostatic rate performance test: the dentifrices prepared in examples 1 to 4 were added to a petri dish containing streptococcus group a, streptococcus anaerobicus, staphylococcus epidermidis, neisseria and lactobacillus in equal amounts, respectively, and the bacteriostatic rates of the dentifrices against the above bacteria were measured, and the results are shown in table 1,

table 1. test results:

as can be seen from Table 1, the antibacterial rates of the dentifrices prepared in the embodiments 1-4 of the invention on Streptococcus A, Streptococcus anaerobicus, Staphylococcus epidermidis, Neisseria and Lactobacillus all reach more than 97%, and the dentifrices have good antibacterial effects.

Performance test 2-tooth cleaning and whitening test: the whitening degree and cleanliness of teeth of a specific population who yellowed the teeth were measured on days 5, 10, 20 and 30 by continuously using the dentifrices prepared in examples 1 to 4 for 1 month, and the results are shown in Table 2,

table 2. teeth cleaning and whitening test results:

as can be seen from table 2, the dentifrices prepared in examples 1 to 4 of the present invention have superior tooth cleaning and whitening effects.